Method of controlling the diameter and wall thickness of vinylidene chloride polymerfilm tubes



Feb. 13, 1951 2,541,064

- C. R. IRONS METHOD OF CONTROLLING THE DIAMETER AND WALL THICKNESS OF VINYLIDENE CHLORIDE POLYMER FILM TUBES Filed Aug. 11, 1948 JNVENTOR. Carr0///?. #003 Patented Feb. 13, 1951 UNITED STATES PATENT OFFICE.

Garroll R. Irons, Midland, Mich., assignor. to The Dow Chemical Company, Midland, Michi, a

corporation of Delaware Application August-11, 1948; Serial No. 43;64'3' 1. Claim. (01. 18 -4.7.5)-

This invention relates toa method of controllihg'th'e diameter and 'th'e wall thickness of vinyliiiene chloride oolymer' tubes, during thecourse rat-their generation in the-production of film.

Crystallinevinylidene chloride polymers havecertain perculiar properties which make necessa-ry*' the use of specialte'chnics'in manufacturing films therefrom. Theprincibal processes for prodiicing strong flexib e films from crystalline vinylldene chlbride" pol'vmers are described by Ti Stephenson in hiscopenclihg application, Serial" No. 721,738; filed- January 13. 1947 now (9? Si Patent No; 2,452,080; and by C. R. Irons ande'z' Ei Sani'brd in copending anplica'tion Serial No. M5 276; filed" September 10, 1945 new U. 8; Patent No; 2448,4533: In outline; theseprocesses comprise the steps of extruding the normally crystallinepolymenin a fused and non-crystalline condition through a' tube-forming orifice downwardlv intoa bathof' cold water to providea': supercooied' and temporarily non-crystalline tube of the polymer; U9S=1Ilg said tube between pinch rolls, and disten'dinq' said tube by fluidpressure from a gas or liqu d" contained withintlie tub e" beyond thepinch rollsto effectrecrystallizat-ion of the oolymer in the form of a thin-- walled" tube which maybe slit to form a film. S'aid processes are ap -lieahle not only to the polymer of vinylidene chloride a one but also to those-vinvlidenechloridecop'olymers which arenormally-crystall'ine, as determinedby'X-ray diffraction studies. They an lv to e trudab e compositions of such normally crystalline pol'vmers, whether plasti'eized or unpl stieizedz All such bodies are referred to herein as normallycrystalline" vinylid'ene chloride polvm'ers.

In: said processes: it' is deemed" a necessary" practice to' fill that oorti'onof theireshlirextruded tube in the" sup'ercooling'bath between the extrusforr orifice and the pinch rolls with an inert liquid canabl'e of" m'oviding enough lubrication to nre ent the internal walls of the tube from adhering to one another" when compressed by the pinch" rolls. The amount of such liquid" in tlic fi'eshly extruded tube has been adjusted; in past" practice; to afiect the diameter and wall thickness oi" the tube: Thus; an increased head of oil" tendsto distend the tube and to red'uce' its" wall thickness, and leads to the" formation of slightly wider and thinner film sheets, while to maintain: aaconstant-- dimensions; in the extruded and stretched Minor variations in operating" conditions-are flected' promptly as variationsin' the finished Another disadvantage of the heretofore. stand-- ard' practices has been the necessity to provide differentextrusion dies foreach significantvariaa tion in the size of film which it: is desiredil toproduce. It would be preferable and muoh more economical if a single extrusion die could beused for the production of a great variety" of widths and thicknesses of film: Ingeneral terms; a tube-forming orifice consists of'a die plate witlr a round opening and a die mandrel disposed cone centrically therewith. The die plateis theileasier to produce and to remove from the apparatus; A simple substitution of one" die plate for an:- other; to provide more or' less clearance from the fixed mandrel (or a similar substitution of one mandrel for another); would be: far more desirable than the practice, now deemedneces sary; of changing both the die' plate: and; the mandrel Whenever a significant changeisu desired in the size of film produced. Since a change only in the clearance between the. die plate and the mandrel results only: in an increase: or decrease in the Wall thickness of the hot tub-em as first extruded", and does not change its internal diameter, accurate control means must be providedlto draw tubes of various thioknessesto' therequired diameter and wall thickness in the supercooled condition, so that, in turn, the recrystallization: step accompanying the final fluid distensioirwill provide the particular width and thickness: (1&- sired in the finished film.

It is among the objects'oi'the present-inv-eirtion to provide a method'for the accurate control of the diameter and" Wall thickness of normally crystallinevinylldene chloride polymer" tubes; during the course of theirgeneration inthe prorduction' of film: A related objectisito provide such a' method whereby any of a wide variety of widths and thicknesses of film may be produced at will using a single. tube-forming die: Another object is to provide such a. method. whereby; with simple substitution of one dieplate for another, and without change of the tubes forming mandrel, a still greater'variety'ofi film sizes maybe produced. A particularobj'eet isto provide a method for' augmenting" thexregu'latory' effect of the column of inert'lubricating liquid normally maintained in that portion 7 of a; fieslilg extruded and non-crystalline tube of normally crystalline: vinylidene chloride polymer between the downwardly directed extrusionorifice andithe -pincl"r; rciisisuhnxersee nil-the: an:

A further object is to effect the desired control as aforesaid through the controlled imposition of pneumatic pressure over the column of inert lubricating fluid in the freshly extruded tube. Additional objects may be pointed out or become apparent from the further description of the invention.

I have found t at the above-noted problems are overcome and that the foregoing objects are attained by the imposition of acontrolled and small amount of pneumatic pressure in that portion of the hot plastic tube of vinylidene chloride polymer between the extrusion orifice and the upper levels of the supercooling bath, over the column of inert lubricating fluid in said tube. The superatmospheric pressure applied is of the order of 0.05 to 2 pounds per square inch, though with some copolymers higher pressures may be required. Such internal pressure, which should be insufficient to rupture the tube, inflates the hot tube immediately outside the extrusion orifice, before upercooling has occurred, and provides a tube, entering the supercooling bath, of any desired tube diameter. This diameter may be'from 1.1 to 4 times that of the extrusion orifice. (After the tube has become supercooled, it will be stretched further, during the crystallization process, to from 3 to 5 times its supercooled diameter, or from about 3 to 20 times the diameter of the extrusion orifice.) With a given tubeforming mandrel in the extrusion head, it is possible, .as well, to extrude the hot plastic tube with walls initially as thin or as thick as desired, by selection of an orifice plate which leaves the desired clearance about the centrally disposed mandrel. The greater the clearance between mandrel and orifice plate, the greater is the wall thickness of the tube as first extruded and, hence, the greater-is the amount of distension which is possible before the tube attains the temporarily set and non-crystalline supercooled condition. The greater the wall thickness of the tube as first extruded, the wider is the possible variation inthe superimposed pneumatic pressure and hence, in the width and thickness of the ultimate stretched andcrystalline film. The use of superatmospheric pneumatic pressure, as described, is amuch more effective means of regulating the dimensions of thetube, before final stretching, than is the previously employed method, in which reliance was hadsolely on the column of inert lubricant for regulation of the dimensions of the freshly extruded and non-crystalline tube. In any specific apparatus, little adjustment is possible in the distance from the extrusion orifice to the bottom of the supercooling bath, and, even though doubling this distance makes possible the use of an oil column of greater height, the resulting additional pressure is applied chiefly at the base of the oilcolumn where the surrounding tube is already supercooled. Hence, unless the oil columnwere to extend above the level of the supercooling liquid, even large variations in its height have little efiect on the diameter and wall thickness of the tube, relative to those now made possible. 7

In normal operation, the oil column extends from the immersed pinch rolls to a level near that of the supercooling bath, leaving an air space within the tube above the oil and beneath the extrusion orifice. In that region the tube is very soft and plastically distensible, as-it is at a fusion temperature when it emerges from the orifice. superatmospheric pressure of 0.65 m l-11d may be obtained by supplyin a r. attle .senting functionally the essential features of the apparatus for carrying out the invention Fig. 2 is a fragmentary view showing the relative shape and size of the film if less air pressure is used than shown in Fig. 1;'and,

Fig. 3 is a similar fragmentary view showing the relative effect of using more air pressure than shown in Fig. 1.

A normally crystalline vinylidene chloride polymer H is fused and forwarded by a conveyor screw i2 in the barrel [3 of a plastics extruder. The fused polymer i i is passed into a downwardly directed extrusion head 54 wherein the hot polymer ii flows around a centrally disposed mandrel It. The polymer it then flows through the tube-forming orifice it, which is iormed by die plate G7 which is attached to the lower face of head l4 and has a circular hole therein of slightly greater diameter than that of the concentrically mounted mandrel E5; The so-extruded polymer emerges from orifice it as a hot and very plastic tube 8 with Walls several times the thickness of the desired final film. Tube 58 is passed info a body of cold water at a supercooling temperature, and is fed-betweenpinch rolls 28 or,

equivalent constricting means, thence around guide roll 23, and finally through pinch rolls 22 and 23. The tube-forming mandrel it is axially bored and is connected at its upper end With a fluid inlet tube 24, through which oil or other. inert lubricating liquid 25 is admitted to that por-'. tion of tube 58 which is in the supercooling bath l9 above the constricting means 2%. That portion of tube it between rolls 22 and 23 is inflated with enough-air to distend'the tube radiallyas far as possible. This condition of inflation is recognized by the fact that the addition of further quantities of air to bubble 26 results in no further radial distension but rather in a length-- ening of the bubble and movement of stretching zone A toward the pinch rolls 22. Rolls 20, 2|, and 22 are set to operate at essentially the same peripheral speed, and this is adjusted to be no less than, and not over 10 per centgreater than the linear rate of extrusion of tube l8 from;

distension of the hot and freshly extruded tube I8 is very small, a low pressure relief valve 29 is attached to line 2'! to assure maintenance of the required low pressure inside the hot tube l8. Valve 29 may be simply constructed and may consist conveniently of a tube 35, dependent from and in open communication with the air inlet tube 2i, dipping into a body of water 35 or'oth'er light i o v r ble death wh ter naoe erations, the liquid 3| is withdrawn from around tube 39, and air, admitted through valve 28 is blown out through tube 39, the oil inlet valve 32 on line 24 being closed. Valve body 29, containing fluid 3| of known density is gradually raised over the end of relief tube 39, forming a hydrostatic head which determines accurately the pressure under which air is admitted to the plastic tube l8. When the right pressure is attained to distend tube It to the desired diameter and wall thickness, the depth of immersion of tube 30 in fluid 3| is measured, and this head of liquid is maintained. At ordinary room temperature, each foot of water exerts a pressure of about 0.43 pound per square inch, and any desired pressure from a fraction of an ounce to several pounds can be obtained readily by variation of the hydrostatic head. It is convenient to make the body of valve 29 of a glass cylinder having a visible scale thereon so that the depth to which tube 30 penetrates the water, alcohol, oil or similar light fluid therein may be measured accurately. The air pressure through valve 28 must always exceed the hydrostatic head of the liquid 3|, to prevent underinfiation of the hot plastic tube I8. The excess air so-supplied through valve 28 is vented through fluid 3! in relief valve 29. Thus, both overinflation and underinflation of tube I8 are prevented, and constant conditions prevail in the critical operation of adjusting the extruded tube 58 to the required diameter and thickness.

Through the use of the herein-described invention, it has become possible to produce film tubes of vinylidene chloride-vinyl chloride crystalline copolymers ranging from about 2.5 to 9 inches in diameter from a small extruder having a tubeforming orifice 0.87 inch in diameter, and with clearances between mandrel and die plate of from 0.030 to 0.060 inch, using a hydrostatic head of 2 to 5 inches of water on the air used to stretch the hot tube just below the orifice. In prior practice, a 3-inch or larger extruder has been necessary to produce a 9-inch film tube, and a series of smaller extruders (or orifices) has been needed to make the smaller tubes.

I claim:

In a method of making film from a normally crystalline vinylidene chloride polymer, wherein the polymer is fused, extruded in tubular form downwardly through air into a supercooling bath, constricted when supercooled beneath the surface of the bath, and thereafter stretched externally of the bath to effect recrystallization, a reduction in wall thickness and an increase in tube diameter, and wherein a column of inert lubricating liquid is maintained in that portion of the non-crystalline tube between the submerged constricting means and the extrusion orifice, the improvement which consists in providing and maintaining a constant superatmospheric pneumatic pressure suflicient to distend but insufiicient to rupture the tube within that part of the hot, freshly extruded non-crystalline tube between the extrusion orifice and the said column of lubricating liquid, the said pneumatic pressure applied over the column of lubricating liquid being the only means used to regulate the wall thickness and diameter of the tube before it is supercooled.

CARROLL R. IRONS.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS Number Name Date 2,070,247 Weingand et al Feb. 9, 1937 2,176,925 Reichel et al Oct. 24, 1939 2,452,080 Stephenson Oct. 26, 1948 2,461,975 Fuller Feb. 15, 1949 2,461,976 Schenk Feb. 15, 1949 

